CN106404765B - The preparation method of silver-colored gold-covered nano stick colorimetric probe and its method for detecting copper ion - Google Patents
The preparation method of silver-colored gold-covered nano stick colorimetric probe and its method for detecting copper ion Download PDFInfo
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Abstract
The preparation method of silver-colored gold-covered nano stick colorimetric probe and its method for detecting copper ion, the preparation method of the silver gold-covered nano stick colorimetric probe, comprising the following steps: (1) seed synthesizes；(2) seed growth；(3) centrifugal purification gold nanorods；(4) synthesis of silver-colored gold-covered nano stick colorimetric probe.The invention also includes the methods of silver-colored gold-covered nano stick colorimetric probe detection copper ion.Silver gold-covered nano stick colorimetric probe prepared by the present invention has good selectivity copper ion, and detection method high sensitivity, open hole detection copper ion concentration has reached 0.1 nmol/L, and the detection limit of colorimetric determination copper ion reaches 0.001 nmol/L；Method is easy to operate, quick, does not need the large-scale instrument by complex and expensive, low in cost, it can be achieved that open hole detection, is suitable for large-scale field quick detection.
Description
Technical field
The present invention relates to the technical fields of copper ion detection, more particularly, to a kind of system of silver-colored gold-covered nano stick colorimetric probe
The method of Preparation Method and its etching reaction detection copper ion.
Background technique
With the continuous development of electronic technology, the demand of global metallic copper also steady growth.To residues such as smelting, mining
It is improper to handle the pollution for causing environment, it constantly attracts much attention in recent years.People have confirmed the mistake of Copper in Body ion
Amount enrichment can cause the damage of nervous system and urinary system.Environmental Protection Agency (EPA) suggestion, copper in drinking water ion
Content should be lower than about 20 μm of ol/L of 1.3 mg/kg().It is, in general, that passing through the precision instrument such as mass spectrum, atom light in laboratory
It is all very simple that spectrum, voltammetry etc., which detect the even lower copper ion of this content,.But it due to these methods or depends on
Large-scale instrument and equipment or shortage selectivity, so that detection quickly on the spot cannot be carried out to the copper ion in environmental water sample.Cause
This, the detection probe and detection method for developing quick, cheap, reliable, high sensitivity the copper ion of one kind are necessary.
Summary of the invention
The technical problem to be solved by the present invention is to, overcome the deficiencies of the prior art and provide it is a kind of quickly, cost is relatively low,
Reliably, the preparation method of with higher sensitivity silver-colored gold-covered nano stick colorimetric probe and its method for detecting copper ion.
The technical solution used to solve the technical problems of the present invention is that
The preparation method of the silver-colored gold-covered nano stick colorimetric probe of the present invention, comprising the following steps:
(1) seed synthesizes: in serum bottle, chlorauric acid solution and CTAB(cetyl trimethylammonium bromide is added) it is molten
Liquid, is added sodium borohydride solution under constant stirring, and solution rapidly goes to dark brown, is further continued for stirring 2min~10min, finally puts
Enter to stand 1~3 h in 28~30 DEG C of water-baths to get seed solution is arrived；Wherein, the gold chloride in chlorauric acid solution and CTAB are molten
The molar ratio of CTAB in liquid is 1:300~500；The sodium borohydride in gold chloride and sodium borohydride solution in chlorauric acid solution
Molar ratio be 1:2.3~2.8；
Further, in step (1), the molar concentration of seed is 0.92~1.15 μm of ol/L in gained seed solution.
(2) seed growth: in another serum bottle, chlorauric acid solution, CTAB solution, silver nitrate solution is sequentially added and is resisted
Bad hematic acid solution is eventually adding the seed solution being prepared in step (1), continues to stir 2min~10min, place into 28~
30min~3h is stood in 30 DEG C of water-baths, obtains red solution, as gold nanorods solution；Wherein, the chlorine gold in chlorauric acid solution
Acid with CTAB solution in CTAB, the silver nitrate in silver nitrate solution, the ascorbic acid in ascorbic acid solution, in seed solution
Seed molar ratio be 1:180~500:0.18~0.25:0.800~1.2:0.000005~0.000007.
(3) purifying of gold nanorods: the gold nanorods solution centrifugal purification that will be prepared in step (2) obtains Jenner
Rice stick；
(4) synthesis of silver-colored gold-covered nano stick: the gold nanorods that purifying obtains in step (3) are added in CTAB solution and are shaken
Uniformly；Then ascorbic acid solution and silver nitrate solution is added, is uniformly mixed；It adds NaOH solution and adjusts pH value to 8~9,
Start coating reaction；It is finally putting into 28~30 DEG C of water-baths and stands 20~24 h to get molten to silver-colored gold-covered nano stick colorimetric probe
Liquid.Wherein, gold nanorods and CTAB, the ascorbic acid in ascorbic acid solution, the nitre in silver nitrate solution in CTAB solution
Sour silver, NaOH in NaOH solution molar ratio be 1:150000~200000:1800~2100:600~850:15000~
20000。
Further, in each step, the molar concentration of the chlorauric acid solution is 20~50mmol/L.The CTAB(ten
Six alkyl trimethyl ammonium bromides) solution molar concentration be 0.05~0.15mol/L.The molar concentration of the sodium borohydride solution
For 0.10~0.12 mol/L.The molar concentration of the silver nitrate solution is 0.01~0.02mol/L.The ascorbic acid solution
Molar concentration be 0.10~0.15 mol/L.The molar concentration of the NaOH solution is 0.1~0.5 mol/L.
Further, in step (1), when sodium borohydride solution is added, it is rapidly added the new sodium borohydride solution prepared and iced.
Further, in step (3), the centrifugal purification, revolving speed is 8000~12000r/min, temperature is 25~30 DEG C
10~30min of lower centrifugation.The molar concentration of gold nanorods is 0.25~0.30 μm of ol/L after centrifugal purification.
Further, in step (4), the molar concentration of silver-colored gold-covered nano stick colorimetric probe solution is 0.04~0.05 μm of ol/
L。
The method of the silver-colored gold-covered nano stick colorimetric probe detection copper ion of the present invention, comprising the following steps:
Centrifuge tube is taken, 150~300 preferred pH=5.4 μ L Tris-HCL(are added) buffer solution, 150~500 μ L matter
The silver-colored gold-covered nano stick colorimetric probe solution of Tween-20 solution and 600~800 μ L preparation that amount concentration is 1~3% (preferably rubs
Your concentration is 0.04~0.05 μm of ol/L), it is uniformly mixed, adds the Na of 25~50 μ L, 50~100 mmol/L2S2O3It is molten
Then 500~1000 μ L testing sample solutions are added in liquid, be finally placed in 20~25 DEG C of constant temperature oscillators and shake 30 min~1
The UV-Vis spectrum change of h, the variation of observing response solution colour or detection solution, the presence of qualitative or quantitative analysis copper ion
Or content.
In the technical solution of the present invention, if reaction solution color is shoaled by blue-green, copper is contained in testing sample solution
Ion, and the concentration of copper ion is greater than or equal to 0.1 nmol/L in solution, if desired quantitative analysis detects in mixed solution
UV-Vis spectrum change determines the concentration of copper ion in solution；If the reaction color does not change, illustrate testing sample solution
There is no the concentration of copper ion in copper ion or solution less than 0.1 nmol/L, if desired quantitative analysis detects in mixed solution
Ultra-violet absorption spectrum variation, determines the concentration of copper ion in solution or whether there is or not copper ions.
In the above-mentioned technical solutions, it in the quantitative analysis, establishes standard curve and carries out quantitative detection, including following step
It is rapid:
(1) prepare the copper ion ultra-pure water solution of various concentration, wherein the concentration of copper ion is respectively as follows: 0,0.001,
0.01,0.1,1,10,100,200,400,600,800,1000,1200,2000 nmol/L；
(2) centrifuge tube for taking 14 5 mL is separately added into 160 μ L Tris-HCL buffer solutions (preferably pH=5.4), 160
The silver-colored gold-covered nano stick colorimetric probe solution of Tween-20 solution and 748 μ L preparation that μ L mass concentration is 1% is (preferably mole
Concentration is 0.04~0.05 μm of ol/L), it is uniformly mixed, adds the Na of 32 μ L, 50 mmol/L2S2O3Solution, then toward not
It is separately added into the copper ion ultra-pure water solution of 500 μ L various concentrations in same centrifuge tube, is finally placed in 20 DEG C of constant temperature oscillators
The h of 30 min~1 is shaken, the UV-Vis spectrum change of its mixed solution is measured.Using the shift value of maximum absorption band as ordinate,
Copper ion concentration is that abscissa draws standard curve, in 0.001-1200 nmol/L Cu2+In range, linear equation be Y=
0.1591X+7.348, linearly dependent coefficient are 0.99314(referring to Fig. 1), it can be used for the quantitative detection of copper ion.
Research has shown that in the technical solution of the present invention, silver-colored gold-covered nano stick colorimetric probe etching reaction detects copper ion
Method, detection range are as follows: 0.001~1200 nmol/L(is referring to attached drawing 2).
Design principle and theoretical basis of the invention:
(1) it is used as a kind of novel composite nano material, the gold nanorods (Au@AgNRs) of silver cladding are same as AuNRs, still
So remain distinctive optical property.But it is compared to common AuNRs, Au@AgNRs is presented with the variation of silver thickness
Different colors and longitudinal absorption peak generate corresponding blue shift (by thin to the thick light gray, blue-green, purplish red of showing respectively out
Color even shiny red).
(2) Cu is utilized2+In S2O3 2–Special catalytic action in-Ag etching system develops a kind of novel label-free colorimetric inspection
Survey Cu in water environment2+Method.As shown in Fig. 3, in no Cu2+In the presence of colloidal sol color and SPR absorption only slightly change
Become, this is because the complexing of Ag and S element, has the surface@AgNRs Au in the presence of dissolved oxygen to form Ag (S2O3)2 3–Compound,
The change that this will cause the oligodynamical of surface silver layer and SPR absorbs, while also preventing the further progress of etching reaction.But
It is, when there is Cu2+It is present in S2O3 2–When-Au@AgNRs sol system, silver-colored thickness of the shell is substantially reduced, and is inhaled along with UV, visible light
Receive the change of spectrum.Cu2+Very strong catalytic action is dissolved with to silver, in Cu2+And S2O3 2-It, can be by silver-colored oxygen when existing simultaneously
It is melted into Ag (S2O3)2 3–, and Cu (S2O3)3 5–Oxygen can be still dissolved and be oxidized to Cu2+.Therefore, in S2O3 2-- Au@AgNRs sol body
Cu is added in system2+, Au@AgNRs silver thickness is substantially reduced, and SPR absorption peak red shift is changed by the displacement at maximum absorption band
Become, is able to achieve Cu in water environment2+Quantitative detection.
(3) selectivity test:
13 5 mL centrifuge tubes are taken, the Tris-HCL buffer solution of 160 μ L, the Tween-20 of 160 μ L1% are separately added into
Solution and 748 μ L silver gold-covered nano stick colorimetric probe solution, 32 μ L, 50 mmol/L Na2S2O3Solution is then respectively adding
500 μ L ultrapure waters, the potassium chloride of 1000 nmol/L, sodium chloride, calcium chloride, magnesium chloride, zinc nitrate, chromium chloride, manganese nitrate,
Iron chloride, plumbi nitras, cobalt chloride, mercury chloride, 200 nmol/L copper chloride, be finally placed in 20 DEG C of constant temperature oscillators and shake 30
The h of min~1 measures the UV-Vis spectrum of its mixed solution, the difference between observation and comparison, referring to attached drawing 4.
As shown, only 200 nmol/L Cu2+In the presence of can just cause the increase of absorption maximum peak shift, S2O3 2–-
Au@AgNRs reaction system color is substantially change.Therefore it can prove that the sensor has good selection to copper ion
Property.
The beneficial effects of the present invention are:
(1) silver-colored gold-covered nano stick colorimetric probe prepared by the present invention has good selectivity copper ion, with other from
Son is compared, and only copper ion, which can be realized, accelerates the catalysis of etching system and significant ultravioletvisible absorption and color is caused to change
Become.
(2) detection method high sensitivity of the invention, open hole detection copper ion concentration have reached 0.1 nmol/L, colorimetric method
The detection limit of detection copper ion reaches 0.001 nmol/L.
(3) detection method of the invention is easy to operate, quick, does not need the large-scale instrument by complex and expensive, at low cost
It is honest and clean, it can be achieved that open hole detection, be suitable for large-scale field quick detection.
Detailed description of the invention
Fig. 1 is S2O3 2-When various concentration copper ion being added in-Au@AgNRs solution, UV-Vis changes in spectrogram most
It is displaced and the canonical plotting of linear relationship between different copper ion concentrations at big absorption peak；
Fig. 2 is S in various concentration copper ion2O3 2-The UV-Vis of-Au@AgNRs solution changes spectrogram；
Fig. 3 is the sensor mechanism that copper ion catalysis etches silver-colored gold-covered nano stick colorimetric probe；
Fig. 4 is the UV-Vis variation spectrogram that silver-colored gold-covered nano stick colorimetric probe is added in different metal ions.
Specific embodiment
In order to preferably explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
The contents of the present invention are not limited solely to following embodiment.
Embodiment 1
The preparation method of the silver gold-covered nano stick colorimetric probe of the present embodiment, comprising the following steps:
(1) seed synthesizes: in 25 mL serum bottles, the chlorauric acid solution and 4 of 40.5 μ L, 0.02428 mol/L is added
The CTAB solution of 0.1 mol/L of mL is rapidly added new 24.5 μ L, the 0.1 mol/L boron hydrogen prepared and iced under constant stirring
Change sodium solution, solution rapidly goes to dark brown, continues to stir 2 min, is finally putting into 28 DEG C of water-baths and stands 2h to get to seed
Solution；
The molar concentration of seed is 0.98 μm of ol/L in gained seed solution.
(2) seed growth: in another 25 mL serum bottle, the gold chloride for sequentially adding 206 μ L0.02428 mol/L is molten
Liquid, 100 mmol/L of the CTAB solution of 10 mL, 0.1 mol/L, the silver nitrate solution of 100 μ L, 10 mmol/L and 52.5 μ L
Ascorbic acid solution, the 30 μ L of seed solution then plus in step (1) being prepared, continue stir 2 min, place into 28
1h is stood in DEG C water-bath, obtains red solution, as gold nanorods solution；
(3) purifying of gold nanorods: the gold nanorods solution of synthesis is put into centrifuge tube, is centrifuged with supercentrifuge pure
Change (10000 r/min of revolving speed, 10 min of centrifugation time).Centrifugal process temperature is set as 25 DEG C, and CTAB crystallization is prevented to be precipitated, in order to avoid
Influence gold nanorods isolates and purifies efficiency；The molar concentration of gold nanorods is 0.28 μm of ol/L after centrifugal purification.
(4) synthesis of silver-colored gold-covered nano stick: 2 mL, 100 mmol/L is added in the 4 mL gold nanorods that purifying is obtained
It is shaken in CTAB solution uniform；Then 10 mmol/L nitric acid of 22 μ L, 100 mmol/L ascorbic acid solution and 85 μ L is added
Silver-colored solution is uniformly mixed；It is 8.5 that the NaOH solution for adding 200 μ L, 0.1 mol/L, which adjusts pH value, starts coating reaction.
It is finally putting into 30 DEG C of water-baths and stands 20 h to get silver-colored gold-covered nano stick colorimetric probe solution is arrived, silver-colored gold-covered nano stick colorimetric is visited
The molar concentration of needle solution is 0.047 μm of ol/L.
The method of the silver gold-covered nano stick colorimetric probe detection copper ion of the present embodiment, comprising the following steps:
5 mL centrifuge tubes are taken, 160 μ L Tris-HCL buffer solutions (pH=5.4) are added, 160 μ L mass concentrations are 1%
Tween-20 solution and 748 μ L silver gold-covered nano stick colorimetric probe solution are uniformly mixed, add 32 μ L, 50 mmol/L
Na2S2O3Then 500 μ L testing sample solutions are added in solution, be finally placed in 20 DEG C of constant temperature oscillators and shake 1 h, and observation is anti-
Solution colour is answered to change, the presence of qualitative analysis copper ion；Or detection solution UV-Vis spectrum change, quantitative analysis copper from
The content of son.
Claims (6)
1. a kind of preparation method of silver gold-covered nano stick colorimetric probe, which comprises the following steps:
(1) seed synthesizes: in serum bottle, chlorauric acid solution and CTAB solution is added, sodium borohydride is added under constant stirring
Solution, solution rapidly go to it is dark brown, be further continued for stirring 2min~10min, be finally putting into 28~30 DEG C of water-baths stand 1~3
H to get arrive seed solution；
(2) in another serum bottle, chlorauric acid solution, CTAB solution, silver nitrate solution and Vitamin C seed growth: are sequentially added
Acid solution is eventually adding the seed solution being prepared in step (1), continues to stir 2min~10min, places into 28~30 DEG C
30min~3h is stood in water-bath, obtains red solution, as gold nanorods solution；
It is gold chloride in chlorauric acid solution and the CTAB in CTAB solution, the silver nitrate in silver nitrate solution, anti-in step (2)
Ascorbic acid in bad hematic acid solution, the seed in seed solution molar ratio be 1:180~500:0.18~0.25:0.800
~1.2:0.000005~0.000007；
(3) purifying of gold nanorods: the gold nanorods solution centrifugal purification that will be prepared in step (2) obtains gold nanorods；
(4) it is equal that concussion in CTAB solution the synthesis of silver-colored gold-covered nano stick: is added in the gold nanorods that purifying obtains in step (3)
It is even；Then ascorbic acid solution and silver nitrate solution is added, is uniformly mixed；It adds NaOH solution and adjusts pH value to 8~9, open
Dynamic coating reaction；It is finally putting into 28~30 DEG C of water-baths and stands 20~24 h to get molten to silver-colored gold-covered nano stick colorimetric probe
Liquid；
In step (1), the molar ratio of the CTAB in gold chloride and CTAB solution in chlorauric acid solution is 1:300~500；Chlorine gold
The molar ratio of the sodium borohydride in gold chloride and sodium borohydride solution in acid solution is 1:2.3~2.8；In gained seed solution
The molar concentration of seed is 0.92~1.15 μm of ol/L；
CTAB, the ascorbic acid in ascorbic acid solution, silver nitrate solution in step (4), in gold nanorods and CTAB solution
In silver nitrate, NaOH in NaOH solution molar ratio be 1:150000~200000:1800~2100:600~850:
15000~20000；The molar concentration of gained silver gold-covered nano stick colorimetric probe solution is 0.04~0.05 μm of ol/L；
In each step, the molar concentration of the chlorauric acid solution is 20~50mmol/L；The molar concentration of the CTAB solution is
0.05~0.15mol/L；The molar concentration of the sodium borohydride solution is 0.10~0.12 mol/L；The silver nitrate solution
Molar concentration is 0.01~0.02mol/L；The molar concentration of the ascorbic acid solution is 0.10~0.15 mol/L；It is described
The molar concentration of NaOH solution is 0.1~0.5 mol/L.
2. the preparation method of silver gold-covered nano stick colorimetric probe according to claim 1, which is characterized in that in step (1),
When sodium borohydride solution is added, it is rapidly added the new sodium borohydride solution prepared and iced.
3. the preparation method of silver gold-covered nano stick colorimetric probe according to claim 1 or 2, which is characterized in that step (3)
In, the centrifugal purification is centrifuged 10~30min in the case where revolving speed is 8000~12000r/min, temperature is 25~30 DEG C；It is centrifuged pure
The molar concentration of gold nanorods is 0.25~0.30 μm of ol/L after change.
4. a kind of method of gold-covered nano stick colorimetric probe detection copper ion silver-colored as obtained by one of claim 1-3, special
Sign is, comprising the following steps:
It takes centrifuge tube, is added 150~300 μ L Tris-HCL buffer solutions, 150~500 μ L mass concentrations are 1~3% to spit
The silver-colored gold-covered nano stick colorimetric probe solution of warm -20 solution and 600~800 μ L preparation, is uniformly mixed, adds 25~50 μ
The Na of 50~100 mmol/L of L2S2O3Then solution is added 500~1000 μ L testing sample solutions, is finally placed in 20~25
Shake the h of 30 min~1 in DEG C constant temperature oscillator, the UV-Vis spectrum of the variation of observing response solution colour or detection solution becomes
Change, the presence or content of qualitative or quantitative analysis copper ion.
5. the method for silver gold-covered nano stick colorimetric probe detection copper ion according to claim 4, which is characterized in that described
In quantitative analysis, establishes standard curve and carries out quantitative detection, comprising the following steps:
(1) prepare the copper ion ultra-pure water solution of various concentration, wherein the concentration of copper ion is respectively as follows: 0,0.001,0.01,
0.1,1,10,100,200,400,600,800,1000,1200,2000 nmol/L；
(2) centrifuge tube for taking 14 5 mL is separately added into 160 μ L Tris-HCL buffer solutions, 160 μ L mass concentrations are 1%
Tween-20 solution and 748 μ L preparation silver-colored gold-covered nano stick colorimetric probe solution, be uniformly mixed, add 32 μ L 50
The Na of mmol/L2S2O3Solution, the copper ion that 500 μ L various concentrations are then separately added into different centrifuge tubes are ultrapure water-soluble
Liquid is finally placed in 20 DEG C of constant temperature oscillators and shakes the h of 30 min~1, measures the UV-Vis spectrum change of its mixed solution；With
The shift value of maximum absorption band is ordinate, and copper ion concentration is that abscissa draws standard curve, in 0.001-1200 nmol/L
Cu2+In range, linear equation is Y=0.1591X+7.348, linearly dependent coefficient 0.99314, the quantitative inspection for copper ion
It surveys.
6. the method for silver gold-covered nano stick colorimetric probe detection copper ion according to claim 4 or 5, which is characterized in that
The method of silver-colored gold-covered nano stick colorimetric probe detection copper ion, detection range are as follows: 0.001~1200 nmol/L.
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| CN106984830A (en) * | 2017-05-25 | 2017-07-28 | 上海应用技术大学 | The preparation method of different draw ratio gold nanorods |
| CN107884376A (en) * | 2017-11-21 | 2018-04-06 | 四川师范大学 | Ratiometric fluorescent probe for mercury ion detecting and preparation method thereof |
| CN108687341B (en) * | 2018-04-13 | 2020-06-23 | 华东理工大学 | Preparation method and application of reducing agent-free photoinduced silver-coated gold nano material |
| CN108672716A (en) * | 2018-05-23 | 2018-10-19 | 厦门斯贝克科技有限责任公司 | A kind of preparation method of silver gold-covered nano stick |
| CN110625134B (en) * | 2019-09-17 | 2022-10-28 | 天津工业大学 | Preparation method of anti-counterfeiting film based on double-layer gold nanorods |
| CN110987915B (en) * | 2019-12-03 | 2022-04-01 | 泸州品创科技有限公司 | Method for rapidly identifying Chinese liquor based on gold nanorod colorimetric sensor array |
| CN113084191A (en) * | 2021-04-12 | 2021-07-09 | 杭州苏铂科技有限公司 | Preparation method of silver-coated gold nanorod |
| CN113533252B (en) * | 2021-06-22 | 2022-09-27 | 中山大学 | Sensor based on strong coupling system, preparation method and application thereof |
| CN113510239B (en) * | 2021-07-07 | 2022-12-09 | 黄河科技学院 | Gold nanorod based on silver coating, and preparation method and application thereof |
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